ChemicalBook CAS DataBase List Ethyl 2-chloroacetoacetate

Ethyl 2-chloroacetoacetate synthesis

9synthesis methods

Product Name:Ethyl 2-chloroacetoacetate
CAS Number:609-15-4
Molecular formula:C6H9ClO3
Molecular Weight:164.59

Using ethyl acetoacetate and thionyl chloride as raw materials, the condensation reaction is carried out in the presence of a solvent. The dosage ratio of ethyl acetoacetate, thionyl chloride, and solvent is 1:1.37~2.75:2.31~4.62 by mass, the temperature of the condensation reaction is 75~95°C, and the reaction time is 5.5-9h. After stopping the reaction, evaporate most of the solvent and unreacted thionyl chloride under normal pressure, and then distill the remaining organic phase under reduced pressure to collect the 107-108°C/1.87kPa fraction to obtain Ethyl 2-chloroacetoacetate Products. The solvents used were n-heptane or, dichloroethane or toluene.

141-97-9 Synthesis

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Yield:609-15-4 98.4%

Reaction Conditions:

with sulfuryl dichloride in dichloromethane at 0 - 20;

Steps:

4
The 11.3 g, 84 mmol of thionyl chloride was added dropwise over 30 minutes previously cooled to 0 ° C containing 10 g, 76.9mmol of ethyl acetoacetate in 100 ml methylene chloride solution. After completion of stirring at room temperature overnight, thereaction solution respectively saturated sodium bicarbonate and saturated sodium chloride solution, the organic layer wascollected, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give 12.4 g of pink oil of ethyl 3-acetyl VII chloroacetate, 98.4% yield, 3- acetyl acid ethyl ester VII

References:

Jiangxi Tianren Ecology Co., Ltd.;Nankai University;Chen, Xiaoyan;Liu, Xiping;Fan, Zhijin;Liang, Xiaowen;Li, Yuedong;Mao, Wutao;Li, Juanjuan;Wang, Dun;Wang, Shuhua;Zhou, Lifeng;Ji, Xiaotian;HUA, XUEWEN CN102942565, 2016, B Location in patent:Paragraph 0028-0031; 0087-0088

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141-97-9 Synthesis

141-97-9
785 suppliers
$5.00/25g